CN105348036B - To the continuous production processes and device of benzyl dichloride - Google Patents
To the continuous production processes and device of benzyl dichloride Download PDFInfo
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- CN105348036B CN105348036B CN201510926691.2A CN201510926691A CN105348036B CN 105348036 B CN105348036 B CN 105348036B CN 201510926691 A CN201510926691 A CN 201510926691A CN 105348036 B CN105348036 B CN 105348036B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/10—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms
- C07C17/14—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms in the side-chain of aromatic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of continuous production processes and device to benzyl dichloride, belong to organic chemical synthesis technical field.Device used in the present invention includes head tank, head tank is connected with three-level chlorination tank, secondary chlorination kettle, one-level chlorination tank, knockout drum and rectifying column successively, is to be connected in parallel between one-level chlorination tank and secondary chlorination kettle, between secondary chlorination kettle and three-level chlorination tank；Continuous production processes are to mix paraxylene and ionic-liquid catalyst, then it is passed through chlorine to it under LED/light source irradiation, obtained after three-level chlorination reaction to benzyl dichloride reaction solution, to benzyl dichloride reaction solution after cooling separation, rectification under vacuum, collect cut and obtain to benzyl dichloride.The present invention, which is solved, produces the problem of discontinuous, product yield is low, production cost is high in existing process, with the characteristics of technological process is succinct, with short production cycle, product purity is high, its apparatus structure is simple, easily operated.
Description
Technical field
The present invention relates to a kind of continuous production processes and device to benzyl dichloride, belong to organic chemical synthesis technical field.
Background technology
It is a kind of important chemical raw material to benzyl dichloride, outward appearance is white flaky crystals, as the intermediate of organic synthesis,
Mainly for the manufacture of terephthalyl alcohol, terephthaldehyde's ether, terephthalaldehyde and other dyestuffs, additionally it is possible in the middle of medicine
Body.CN104230653A is disclosed carries out chlorination with paraxylene at 80 DEG C, when being reached in sample to benzyl dichloride content
Stop logical chlorine during 35wt%, then obtained by carrying out flash distillation and rectifying to benzyl dichloride, the technique is to benzyl dichloride conversion ratio
Just flashed and vacuum distillation when reaching 35%, there are problems that conversion rate of products is low, cost.
The content of the invention
It is an object of the invention to provide a kind of continuous production processes to benzyl dichloride, solve to produce in existing process and do not connect
It is continuous, the problem of product yield is low, production cost is high, with the characteristics of technological process is succinct, with short production cycle, product purity is high；
Present invention simultaneously provides the device that it is used.
Continuous production processes of the present invention to benzyl dichloride, are to mix paraxylene and ionic-liquid catalyst,
Then chlorine is passed through to it under LED/light source irradiation, is obtained after three-level chlorination reaction to benzyl dichloride reaction solution, it is anti-to benzyl dichloride
Answer liquid after cooling separation, rectification under vacuum, collect cut and obtain to benzyl dichloride.
Wherein：
Described ionic-liquid catalyst is 1- dodecyl -3- methylimidazole villaumites or 1- butyl -2,3- methylimidazole chlorine
Salt.
Described ionic-liquid catalyst consumption is the 1 ‰ -5 ‰ of paraxylene quality.
Described paraxylene and the mol ratio of chlorine are 1:1.3-2.0.
Described reaction temperature is 110-120 DEG C.
It is described to being 80-90wt% to the content of benzyl dichloride in benzyl dichloride reaction solution.
Described cooling temperature is 85-90 DEG C.
Vacuum during described vacuum distillation is 8mmHg, and the cut temperature of collection is 150-155 DEG C.
Device used in continuous production processes of the present invention to benzyl dichloride, including head tank, head tank is successively
It is connected with three-level chlorination tank, secondary chlorination kettle, one-level chlorination tank, knockout drum and rectifying column, one-level chlorination tank and secondary chlorination kettle
Between, between secondary chlorination kettle and three-level chlorination tank be to be connected in parallel.
Wherein：
Described head tank is connected by inlet valve with three-level chlorination tank, three-level chlorination tank bottom by two grades of reflux pumps with
Secondary chlorination kettle is connected, and secondary chlorination bottom portion is connected by one-level reflux pump with one-level chlorination tank, and knockout drum bottom is by entering
Material pump is connected with rectifying column, and connection condenser at the top of chlorine intake valve, rectifying column is provided with the top of one-level chlorination tank.
The top of described one-level chlorination tank, secondary chlorination kettle and three-level chlorination tank is equipped with overfall；Head tank and three
Between level chlorination tank, between three-level chlorination tank and secondary chlorination kettle, between secondary chlorination kettle and one-level chlorination tank, one-level chlorination tank
Potential difference between knockout drum is 1-3m.
Ionic liquid in the present invention is called " high-temperature fusion salt ", and it has wider liquid temperature scope and good thing
Reason and chemical property, it is non-volatile, nonflammable explosive, do not aoxidize, with higher heat endurance, water and air is stablized, together
When the advantageous characteristic with good solvability, larger polarity and controllability and approximate zero toxicity.
The reaction equation of the present invention is as follows：
The present invention to mainly containing paraxylene in benzyl dichloride reaction solution, to benzyl dichloride and to methyl benzyl chloride, to diformazan
The fusing point of benzene is -48 DEG C, is 98-101 DEG C to the fusing point of benzyl dichloride, and the fusing point to methyl benzyl chloride is 4 DEG C, using each in reaction solution
The fusing point of material is different, by the way of cooling separation, makes to benzyl dichloride with paraxylene and methyl benzyl chloride is separated, point
Paraxylene from after and reactor is entered from knockout drum upper strata to methyl benzyl chloride continue to react, benzyl dichloride enters essence between lower floor
Tower processed is refined, so as to reduce the reaction of the continuation to benzyl dichloride and chlorine, can be played the generation of reduction accessory substance and be improved and receive
The purpose of rate.
Beneficial effects of the present invention are as follows：
The production technology of the present invention is obtained to benzyl dichloride, and fusing point is 98-101 DEG C, and purity is up to more than 99%, with technique
The characteristics of flow is succinct, with short production cycle, cost is low, whole technical process three-waste free discharge, realizes continuous production, simultaneously
The stability of product yield and whole system is improved, its apparatus structure is simple, easily operated.
Brief description of the drawings
Fig. 1 is the structural representation of apparatus of the present invention.
In figure：1st, head tank；2nd, inlet valve；3rd, three-level chlorination tank；4th, two grades of reflux pumps；5th, secondary chlorination kettle；6th, one-level
Reflux pump；7th, one-level chlorination tank；8th, knockout drum；9th, feed pump；10th, chlorine intake valve；11st, condenser；12nd, rectifying column；13rd, overflow
Head piece.
Embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
Device used in the present embodiment as shown in figure 1, head tank 1 successively with three-level chlorination tank 3, secondary chlorination kettle 5, one
Level chlorination tank 7, knockout drum 8 are connected with rectifying column 12, between one-level chlorination tank 7 and secondary chlorination kettle 5, secondary chlorination kettle 5 and three
It is to be connected in parallel between level chlorination tank 3；Head tank 1 is connected by inlet valve 2 with three-level chlorination tank 3, the bottom of three-level chlorination tank 3
It is connected by two grades of reflux pumps 4 with secondary chlorination kettle 5, the bottom of secondary chlorination kettle 5 passes through one-level reflux pump 6 and one-level chlorination tank 7
It is connected, the bottom of knockout drum 8 is connected by feed pump 9 with rectifying column 12, the top of one-level chlorination tank 7 is provided with chlorine intake valve 10,
The top of rectifying column 12 connection condenser 11；The top of one-level chlorination tank 7, secondary chlorination kettle 5 and three-level chlorination tank 3 is equipped with overflow
Mouthfuls 13, between head tank 1 and three-level chlorination tank 3, between three-level chlorination tank 3 and secondary chlorination kettle 5, secondary chlorination kettle 5 and one-level
Potential difference between chlorination tank 7, between one-level chlorination tank 7 and knockout drum 8 is 1m.
Concrete operations are as follows：
(1) paraxylene and 1- dodecyl -3- methylimidazole villaumites are added in head tank 1, wherein 1- dodecyls -3-
Methylimidazole villaumite is the 1 ‰ of paraxylene quality, opens the inlet valve 2 of the bottom of head tank 1 successively to three-level chlorination tank 3, two
Level chlorination tank 5 and one-level chlorination tank 7 are flowed into and fed between uniform material, reactors at different levels by overfall 13, are then beaten
The material opened in the chlorine intake valve 10 at the top of one-level chlorination tank 7, one-level chlorination tank 7 is reacted in LED/light source irradiation, is reacted
Temperature is 110 DEG C；
(2) tail gas and unreacted chlorine produced in one-level chlorination tank 7 is by one-level reflux pump 6 by secondary chlorination kettle
5 bottom is reacted after entering, and reaction temperature is the tail gas and unreacted chlorine produced in 110 DEG C, secondary chlorination kettle 5
Reacted further through two grades of reflux pumps 4 after the bottom entrance of three-level chlorination tank 3, reaction temperature is 110 DEG C, when one-level chlorination
Kettle 7 to being 80wt% to the content of benzyl dichloride in benzyl dichloride reaction solution when, benzyl dichloride reaction solution is entered by overfall 13
Knockout drum 8 carries out cooling layered shaping, and temperature is maintained at 85 DEG C, and upper solution is returned in head tank 1, and lower floor is thick to benzyl dichloride
Product；
(3) benzyl dichloride crude product will be added in rectifying column 12 by feed pump 9, vacuum distillation is carried out under 8mmHg, received
The cut of 150-155 DEG C of collection, is obtained to benzyl dichloride.
As a result show：Obtain to benzyl dichloride content 99.11%, fusing point is 98.5-100.9 DEG C, and the reaction time is than interval
Reaction time saves 10%, and the unit consumption of product of successive reaction is than intermittent reaction reduction by 15%.
Embodiment 2
Such as embodiment 1 of device used in the present embodiment, except that between head tank 1 and three-level chlorination tank 3, three-level
Between chlorination tank 3 and secondary chlorination kettle 5, between secondary chlorination kettle 5 and one-level chlorination tank 7, one-level chlorination tank 7 and knockout drum 8 it
Between potential difference be 2m.
Concrete operations are as follows：
(1) paraxylene and 1- dodecyl -3- methylimidazole villaumites are added in head tank 1, wherein 1- dodecyls -3-
Methylimidazole villaumite be paraxylene quality 5 ‰, then from the bottom of head tank 1 inlet valve 2 successively to three-level chlorination tank 3,
Secondary chlorination kettle 5 and one-level chlorination tank 7 are flowed into be fed between uniform material, reactors at different levels by overfall 13, then
The material opened in the chlorine feed valve 10 at the top of one-level chlorination tank 7, one-level chlorination tank 7 is reacted in LED/light source irradiation, instead
It is 120 DEG C to answer temperature；
(2) tail gas and unreacted chlorine produced in one-level chlorination tank 7 is by one-level reflux pump 6 by secondary chlorination kettle
5 bottom is reacted after entering, and reaction temperature is the tail gas and unreacted chlorine produced in 120 DEG C, secondary chlorination kettle 5
Reacted further through two grades of reflux pumps 4 after the bottom entrance of three-level chlorination tank 3, reaction temperature is 120 DEG C, when one-level chlorination
Kettle 7 to being 90wt% to the content of benzyl dichloride in benzyl dichloride reaction solution when, benzyl dichloride reaction solution is entered by overfall 13
Knockout drum 8 carries out cooling layered shaping, and temperature is maintained at 90 DEG C, and upper solution is returned in head tank 1, and lower floor is thick to benzyl dichloride
Product；
(3) benzyl dichloride crude product will be added in rectifying column 12 by feed pump 9, vacuum distillation is carried out under 8mmHg, received
The cut of 150-155 DEG C of collection, is obtained to benzyl dichloride.
As a result show：Obtain to benzyl dichloride content 99.32%, fusing point is 98.5-100.6 DEG C, and the reaction time is than interval
Reaction time saves 16%, and the unit consumption of product of successive reaction is than intermittent reaction reduction by 20%.
Embodiment 3
Such as embodiment 1 of device used in the present embodiment, except that between head tank 1 and three-level chlorination tank 3, three-level
Between chlorination tank 3 and secondary chlorination kettle 5, between secondary chlorination kettle 5 and one-level chlorination tank 7, one-level chlorination tank 7 and knockout drum 8 it
Between potential difference be 3m.
Concrete operations are as follows：
(1) paraxylene and 1- butyl -2,3- methylimidazole villaumites are added in head tank 1, wherein 1- butyl -2,3-
Methylimidazole villaumite is the 1 ‰ of paraxylene quality, and then the inlet valve 2 from the bottom of head tank 1 is respectively successively to three-level chlorination
Kettle 3, secondary chlorination kettle 5 and one-level chlorination tank 7 are flowed into be fed between uniform material, reactors at different levels by overfall 13,
Then the material opened in the chlorine feed valve 10 on the top of one-level chlorination tank 7, one-level chlorination tank 7 is carried out instead in LED/light source irradiation
Should, reaction temperature is 120 DEG C；
(2) tail gas and unreacted chlorine produced in one-level chlorination tank 7 is by one-level reflux pump 6 by secondary chlorination kettle
5 bottom is reacted after entering, and reaction temperature is the tail gas and unreacted chlorine produced in 120 DEG C, secondary chlorination kettle 5
Reacted further through two grades of reflux pumps 4 after the bottom entrance of three-level chlorination tank 3, reaction temperature is 120 DEG C, when one-level chlorination
Kettle 7 to being 90wt% to the content of benzyl dichloride in benzyl dichloride reaction solution when, benzyl dichloride reaction solution is entered by overfall 13
Knockout drum 8 carries out cooling layered shaping, and temperature is maintained at 86 DEG C, and upper solution is returned in head tank 1, and lower floor is thick to benzyl dichloride
Product；
(3) benzyl dichloride crude product will be added in rectifying column by feed pump 9, vacuum distillation is carried out under 8mmHg, collected
150-155 DEG C of cut, is obtained to benzyl dichloride.
As a result show：Obtain to benzyl dichloride content 99.28%, fusing point is 98.7-100.6 DEG C, and the reaction time is than interval
Reaction time saves 10%, and the unit consumption of product of successive reaction is than intermittent reaction reduction by 15%.
Claims (5)
1. a kind of continuous production processes to benzyl dichloride, it is characterised in that：Paraxylene and ionic-liquid catalyst are mixed, so
Chlorine is passed through to it under LED/light source irradiation afterwards, is obtained after three-level chlorination reaction to benzyl dichloride reaction solution, benzyl dichloride is reacted
Liquid is collected cut and obtained to benzyl dichloride after cooling separation, rectification under vacuum；
The ionic-liquid catalyst is 1- dodecyl -3- methylimidazole villaumites or 1- butyl -2,3- methylimidazole villaumites, ion
Liquid catalyst consumption is the 1 ‰ -5 ‰ of paraxylene quality, to being 80- to the content of benzyl dichloride in benzyl dichloride reaction solution
90wt%.
2. the continuous production processes according to claim 1 to benzyl dichloride, it is characterised in that：Paraxylene and chlorine rub
You are than being 1:1.3-2.0.
3. the continuous production processes according to claim 1 to benzyl dichloride, it is characterised in that：Reaction temperature is 110-120
℃。
4. the continuous production processes according to claim 1 to benzyl dichloride, it is characterised in that：The temperature that cools is 85-90 DEG C.
5. the continuous production processes according to claim 1 to benzyl dichloride, it is characterised in that：Vacuum during vacuum distillation
For 8mmHg, the cut temperature of collection is 150-155 DEG C.
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| CN201510926691.2A CN105348036B (en) | 2015-12-14 | 2015-12-14 | To the continuous production processes and device of benzyl dichloride |
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| CN201510926691.2A CN105348036B (en) | 2015-12-14 | 2015-12-14 | To the continuous production processes and device of benzyl dichloride |
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| CN105348036A CN105348036A (en) | 2016-02-24 |
| CN105348036B true CN105348036B (en) | 2017-08-25 |
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| CN109336759A (en) * | 2018-12-03 | 2019-02-15 | 山东民基化工有限公司 | Continuously prepare the method and device thereof of chloro-pivalyl chloride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948245A (en) * | 2006-04-14 | 2007-04-18 | 浙江巍华化工有限公司 | Method of producing chlorobenzyl by photochlorination |
| CN104230653A (en) * | 2014-09-22 | 2014-12-24 | 潜江新亿宏有机化工有限公司 | Manufacturing technology of p-xylylene dichloride |
| CN104402698A (en) * | 2014-10-29 | 2015-03-11 | 柳州丰康泰科技有限公司 | 2-(4-methylphenyl)propionic acid syntehsis method |
-
2015
- 2015-12-14 CN CN201510926691.2A patent/CN105348036B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948245A (en) * | 2006-04-14 | 2007-04-18 | 浙江巍华化工有限公司 | Method of producing chlorobenzyl by photochlorination |
| CN104230653A (en) * | 2014-09-22 | 2014-12-24 | 潜江新亿宏有机化工有限公司 | Manufacturing technology of p-xylylene dichloride |
| CN104402698A (en) * | 2014-10-29 | 2015-03-11 | 柳州丰康泰科技有限公司 | 2-(4-methylphenyl)propionic acid syntehsis method |
Non-Patent Citations (2)
| Title |
|---|
| 氯化烷基咪唑: 一种氯气吸收及氯化反应的媒介;施沈一等;《有机化学》;20111231;第31卷(第2期);第227～230页 * |
| 甲苯定向氯化新技术进展;俞志宏等;《化工时刊》;20111031;第25卷(第10期);第49-51页 * |
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Address after: Double Yang Zichuan District 255190 Shandong city of Zibo Province Applicant after: Shandong Kaisheng New Materials Co.,Ltd. Address before: Double Yang Zichuan District 255190 Shandong city of Zibo Province Applicant before: SHANDONG KAISHENG NEW MATERIALS CO., LTD. |
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Inventor after: Wang Ronghai Inventor after: Zhang Liang Inventor after: Liu Song Inventor after: Xue Juqiang Inventor after: Zhang Qingxin Inventor after: Zhang Taiming Inventor after: Bi Yixia Inventor after: Xie Shengbin Inventor after: Jia Yuanchao Inventor after: Han Nannan Inventor after: Shi Yufei Inventor before: Xue Juqiang Inventor before: Wang Ronghai Inventor before: Zhang Qingxin Inventor before: Zhang Taiming Inventor before: Bi Yixia Inventor before: Xie Shengbin |
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